Process for producing intimate mixtures of substances, and for obtaining chemical products therefrom



July 30, 1929. J. w. SPENSLEY PROCESS FOR PRODUCING INTIMATE MIXTURES OF SUBSTANCES AND FOR OBTAINING CHEMICAL PRODUCTS THEREFROI Filed. March 5, 1923 4 Sheets-Sheet 1 lift ml? July 30, 1929. w SPENSLEY 1,722,687

PROCESS FOR PRODUCING INTIMATE MIXTURES OF SUBSTANCES AND'FOR OBTAINING CHEMICAL PRODUCTS THEREFROH v FileQ March 5, 192 5 4 Sheets-Sheet 2 Fig.2.

PROCESS FOR PRODUCING INTIMATE MIXTURES 0F SUBSTANCES July 30, 1929. J. w. SIPENSLIIEY ,7

AND FOR' OBTAINING CHEMICAL PRODUCTS THEREFROM Filed'Mar ch 5, 1923 4 Sheets-Sheet 3 fmw f July 30 1929. w; SPENSLEY 1,722,687

PROCESS FOR PRODUCING'INTIMATE MIXTURES OF SUBSTANCES AND FOR OBTAINING CHEMICAL PRODUCTS THEREFROM Filed March 5, 1923 4 Sheets-Sheet 4 4 (Ittorneg Patented July 30; 1929.

UNITED STATES 1,722,687 PATENT OFFICE,

JACOB WILLIAM SPENSLEY, 0F MANCHESTER,ENGLAND.

PROCESS FOR PRODUCING INTIMATE MIXTURES 0F SUBSTANCES, AND FOR OBTAINING V CHEMICAL PRODUCTS THEREFROM.

Application filed March 5', 1923, Serial No. 623,067, and in Great Britain April 4,1922.

This invention relates to processes for producing intimate mixtures of substances with the object of formingchemical compounds or. mixtures containing products of reaction. The invention depends upon the treatment of materials in a high-speed centrifugal type of mill with intercalating pins mounted upon discs. Various types of intercalating pinned disc mills are known which operate with a beater action 'upon materials fed in at the centre of the discs, and thrown outwardly by centrifugal action. The preferred type of mill for the purposes of the present invention is that set forth in the specification of my British Patent No 186,462wherein the discharge from the rotating pi-n'ned disc can take place all round the circumference The mills of the type referred to, having discs with intercalating pins, can be run up to speeds of about 20,000 feet per minute apd with a minimum peripheral speed of 10,000 feet per min ute at the outermost row of pins or the circumference of the disc carrying the same.

I have now discovered that when liquid mixtures, or solids and semi-solids whether mixed or not withliquids, are passed through such mills, it is possible to effect such intimate mixtures of the ingredients that reactions between them are caused to take place practicallyinstantaneously, which reactions could otherwise only be made to take place in general by the use of long continued heating or long continued agitation, or, both. By the use of the high speed centrifugally fed pinned disc mill in the processes according to this invention the speed at which'the reactions are caused to take place isgreatly increased and the results are substantially improved as compared with results obtainable by other processes hitherto in use. Gases may also enter into the reactions in the mill. When required for any purpose, the mill in which the reactions according this invention are caused I to take place may be heated for exampleby steam'coils or a heating jacket,

In the accompanying drawings Figure 1 is a front view, partly in section, on the line 1--1 of Figure 3;

Figure 2 is aside view, partly in section, on the line 22 of Figure 3, and

Figure 3 is a plan view partly broken away, ofa form of pinned disc mill andjits accessories suitablefor the practice of my invention, and i Figure 4 is an elevation half in section of the mill, apart from its casing. c

In these drawings, Figures 1 and 3 show a form of casing and accessories for, use with the open deliverypinned disc mill, when the gearing is contained. At the top of this shell is aplate y secured by screws oand whose circumference constitutes the "delivery ring Z).

Therotating disc d of the mill is secured to the driven vertical shaft which is carried in ball bearings in a suitable manner in the plate 3 as indicated by way of example.

of lugs 7, four in" the example shown, on the delivery ring 6, and is secured by screws 9 engaging in these lugs. The bottom disc which rotates has concentric rows of upwardly projecting pins upon it, .while the top disc 6 which is stationary has similar concentric rows intercalating with those on the disc (Z. Hitherto, in pinned disc mills the lower disc which rotates,-has always carried the ou ermostrow of pins, this being essential in the case of mills with a tangential discharge in order to insure the throwing out of the ground The stai tionary top disc 0 is suppported by' number,

materials through such discharge.- A feature a of :my disinte rating mill is that it enables me to applyarf additional annular row of pins 2 to the upper fixed disc e, outside the last row of pins on the lower disc at, and so to improve the efficiency of the mill. I find theft with the addition of this row of pins 2,, the material is ground to a greater degree of fineness in one passage through the mill, Without the consumption of appreciably more power, and without any risk of choking the mill owing to the open circumferential discharge. The current of air which the rotation of the lower disc induces through the mill is quite suificientto insure that the material is blown cleanly through the additional outermost row of stationary pins. h is a feed hopperat the centre of the top disc for delivering the ma terials to be treated on to the surface of the rotating disc 0?. I

The mill itself carriedby the standard 4, may be identical with the mill shown in Figures' 1 and 2 of the drawings of British Patent Specification No. 186,462. Its discharge outlet is surrounded by an annular casing or bin 5 which receives the discharged products, and a scraper 6 is caused to move round inside the casing 5, so as to discharge the roducts' through the opening 7 of a chute 8; t 115 chute leadsto the bottom of an elevator 9 for taking away the products to any required point of delivery ina factory. The scraper 6 is driven from the power shaft 10 through belt pulleys 11 and 12, and belt 13, the pulley 12 being on a shaft 14 which carries a worml5." This worm drives worm wheel 16 secured to a sleeve 17 which is revolubly su ported in thetop 24 of the bin 5 and upon t 1e cover 18 of the mill, and carries the scraper 6. The feed hopper 19 for the mill communicates with the interior of this latter through a tubular inlet'20 passing down through the interior of the rwoluble sleeve 17, and into the central aperture of 7 able.

1. Com/man soap Martiactura-A method commonly adopted for making common ghard) soa is to boil in a pan the fatty acids obtained rom fats by splitting them with sulphonated oil to separate the glycerine),

- and to add the alkali such as caustic soda, continuing the boilin for about two days, after which the saponi ed product can be run into frames to sohdify. According to the present invention, the in edients for making the common soap are rought into intimate contact in the mill, and after being passed through the mill any required 'number of times the product is a soap which requires no boiling or other such treatment in order to complete. its manufacture.

.As a practical example of the ingredients which may be used in making a soap the fol lowing may be given: 4 parts by weight of coconut oil and 6 parts by weight of stearine are melted to ether in asuitable pan at a tem-; perature of a out 82 C. 1.5 parts by weight of solid sodium hydrate are dissolved in 11 parts by weight of water, and the solution of sodium hydrate is run into the mill at a uniform s d simultaneously with the hot mixture o coconut oil and stearine, the speed of running in being such that the proportions of the ingredients are in the ratio as above referred to. After passing through the mill once, the product is fed into the same or another mill, and after the second passage throu h the mill the product will be found to be sti l warm. It can be run straightinto fat remains therein, the intimate contact between the particles which is effected by the passage through the mill being suflicient to insure the completion of the reaction. A single high speed mill of the type set forth having a rotating disc about 26 in diameter provided with 87 pins, each one inch in diameter and operated at 27,000 revolutions per minute, thus producing a peripheral speed of 18,368 feet per minute will complete the saponification of one ton of the mixture per hour, allowing for two passages of the mixture through the mill.

2. Soft soap manufactwre.-The method only differs from that set forth abovejn regard-to the ingredients used. These ingredicuts are generally vegetable or animal oil and caustic potash.

As an example of a suitable mixture the following may be given: 8 parts by weight ofolein containing 95% of free fatty acid, and 2 parts by weight of cotton seed oil are heated in a pan to a temperature of about 82 C.', and a solution of caustic potash is made up to'a density of 38 Twaddell. 11.5 parts by weight 'ofthis solution are run into the mill at a uniform rate, while 10 parts by wei ht of the fatty acid are being run in, an saponification is complete after a single'passage through the mill. More water may be used if desired, depending upon the quality of the soap to be made.

3. Manufacture of dry 80a powder.-A

, method commonly adopted hit erto for making dry soap is to mix soda ash with a considerable percentage of water and after the product has set it is groundup to form a fine powder. With-this is mixed in mechanical mixing apparatus .a certain percentage *of disintegrated common soap made by usual methods. The mixture forms a dry soap powder. According to the present invention the ingredients for making the soap itself, and also the soda ash or its equivalent, or even caustic soda, and the necessary amount of water are introduced simultaneously into the high speed centrifugal pinned disc mill,'and are caused to combine during one or more passages through the mill with the formation of a finely disintegrated dry soap powder. A fatty acid is taken in quantity sufiicient in relation to the other in redients to form a dry soap having the required soap content; an amount of soda ash or its equivalent is also taken sufficient, on the one hand, to combine with thefatty acid and to saponify it completely, and, on the other hand, to introduce Y the mill, but at least a superficial layer of soap into the dry soap powder ,the requisite amount of uncombined soda ash to give the soap powder its detergent .action. In the passage of the mixture through the mill the high speed beating action combined with the centrifugal action throwing the materials against and through the spaces between the pins insures that the fatty acid is completely combined with soda to form soap and that the soap so formed is intimately mixed with the rest of the soda ash, the mixture taking up the amount of water with which it will combine so that the product issues as a substantially dry powder.- i

As a practical example of the manufacture of the dry soap the following may be given:

6 parts by weight of palm kernel fatty acid 'may bementioned: An animal fat such as are stirred up with 7 parts by weight of water at a temperature of about C. and the mixture is poured in to the inlet hopper of the mill, while dry soda ash is fed in mechanically at such a rate that about 21 parts by weight of soda ash are introduced while 6 parts by weight of fatty acid and 7 parts by weight of water are being fed in. The product as it leaves the mill is a fine powder which is non-hygroscopic and will therefore remain in packages as a .dry soap powder. The reaction between the fatty acid and the soda ash may not be complete when the product leaves will be formed around each particle of soda ash which has any uncombined fatty acid in contact with it so that no caking together will occur if the saponifying reaction continues after product leaves the mill.

l. Ztlanafacture of edible oiZs (removal of free fatty acid'from oils) .In producing edible oils it is necessary to saponify the fatty acids contained in" the oils, and the usual method of doing this at present is to treat the oils with caustic soda. The result, however, is not only to saponify the fattyacids, but also to saponify an appreciable amount of the neutral fats, so that the yield in edible oils is substantially reduced. According to this invention, soda ash anhydrous Na CO is used, this being mixed with the oil andthe mixture passed through the pinned disc mill.

Only so much of soda ash is added as is theoretically necessary to combine with the fatty acids present, or but a very slight excess of soda ash. Experiments which I have made .As an example of the removal indicate that a very intimate mixture of the soda ash with the fatty acids in the mill .results in the practically complete saponifica- 'tion of the fatty acids, while the neutral fats remain practicallyunsaponified. of free'fatty acid from oils the following may be given: A certain whale oil contains 10.3% of fatty acid which it is desired to remove as far as possible. A solution is made containing 4.3 parts by weight ofsoda ash dissolved in 28 parts by weight of water, .and this is run by Weight of the whale oil to be treated. I The free fatty acid in the Whale oil is saponified I down to 0.5% on a single passage through the mill. Substantially none of the neutral fat in the whale oil will have been attacked by the soda ash in the treatment.

5. Manufacture of lab m'cants and greases.- Solid and semi-solid lubricants or greases such. ashstauffergreases can be made in the mill as follows: Fattyn'iatter is treated in the mill with a neutralizing agent so as to give a saponified product, and this product is afterwards mixed in the mill with a mineral oil, the mixture being subsequently boiled for a short time.

As anexample of the process the following bone grease, or a vegetable fat such as palm oil, stearine or olein, or mixture of these; must 1 be mixed with as nearly as possible the theoretical quantity of the neutralizing agent such as lime or caustic soda, which is required to neutralize or saponify the fatty acids. About 14% of lime may be-needed for example. The fat if solid or semi-solid, may be melted, and the lime may be mixed with it in advance, or the meltedfat may be fed to the high speed centrifugal pinned disc mill at the same time as the lime is fed thereto.

Generally a single passage of the mixture 'it to a finely powdered condition.

- The finely divided product is mixed with mineral oil the amount'of which will vary' according to the quality of the grease required, and the mixture is passed through the high speed centrifugal pinned disc mill or is madetherein by feeding thesolid matter'and mineral oil. simultaneously into the. mill.

Suitable amounts of mineral oil may be such as to give from 16 to 24% of the lime soap in the finished grease. The mixed product discharged from the mill is delivered into pans andis kept boiling therein for say 15 to 30 minutes, or longer as may be required, when it can be run into receptacles ready for sale as a finished grease.

12c The product ,is I

glossy and smooth, that is-to say it is quite free from solid matter or grit, and a substantial saving is'efiecteddn the cost of manufacture owi'nfg to the short time which it occupies as compared with the processeshitherto usual wherein the constituents of the product are all boiled together for several hours,

I find that the neutralizing reactionin the mill is rendered more complete and instani taneous if a small percentage of water is preswith the oil.

cut during the ,saponification. The lime may be moistwhen introduced for example, and in thecase of a lime soap bein first made as above d8SC1lbGd, &b0lll2-2% of water in ,the product is sufiicient. If the fatty acid is neutralized with caustic alkali, a larger percentage of moisture is-desirable, say up to 5% or 7%, according to the required consistency of the final product. Instead of saponifying the fatty matter with the'neutralizing agent first and then mixing in the mineral oil, it is ossible to make a product by mixing all the ingredients together in onepassage through the mill. For example 32 parts by weight of pale stearine may be mixed with 128 parts by weight of a mineral oil such as pale spindle oil, the mixture being heated to about 82 C.

To this mixture may be added before the passage through the mill 4.5 parts by weight of solid sodium hydrate and 6 parts by weight of water, or the solid sodium hydrate and the water may be fed into the mill simultaneously In order that the reaction may be complete it may be necessary to run the mixture two or even three times through the mill.

6. Manufacture of disz'nfectcmta A useful disinfectant preparation can be made by grinding rosin, preferably dry, in the mill, adding oil such as that commonly known as brick oil (which is a crude cresol distillate consisting of phenol and ortho, meta and para cresol,) and running the mixture through the mill, together with enough caustic soda or soda ash for saponification. The product is completed after a few times of passing through the mill.

As a practical example of this it-may be stated that if 18 parts by weight of brick oil, 160 parts by weight of water, 0.5 parts by weight of ground rosin, and enough caustic soda to effect the saponification, are roughly mixed together and the mixture is then passed through the mill say three times, the product is a dense permanent emulsion of the disinfectant in water.

7. Manufacture of size for use in papermaking and s0 f0rth.-For making sizes, rosin is ground dry preferably in a pinned disc mill and is then mixed with a ready-made solution of caustic soda. The 'amount of soda required will vary according to the amount of free rosin which is to be left in the finished size.

rosin is saponified by the caustic soda issues as a semi-solid. The amount of water introduced may be varied according to the stiffness of the roduct required.

8. Manu acture of caustic soda-Methods hitherto employed for making caustic soda involve the a 'tation of soda ash (Na,GO,) .with milk of ime'for long periods, the concentration of'the, resulting solution being The mixture is run through. the mill and the product in which some of the about 10%. According to the present invention a substantially better product of a higher concentration is obtained much more quickly. Milk of lime is prepared by stirring burnt lime with water, and soda ash is also made into a milk with water. These two milky preparations are mixed together and are passed through the high speed centrifugal pinned disc mill any required number of times. The product is then run into a filter press or is treated in a hydro-extractor, and the solution obtained consists of caustic soda of a strength of 20% or above, according to the length of treatment in the mill. The solution can, of

course, be evaporated down to any required strength in evaporating pans, but much time and expense is saved in the evaporation owing to the relatively high initial concentration.

As a practical example the following may be given: 6 parts by weight of lime are slaked with 10 parts by weight of water to form the oneingredient, and 10.5 parts by weight of soda ash are dissolved in 25 parts by weight of water to form the other ingredient. These two ingredients are poured insimultaneously at a rate such that 16 parts by weight of the first are introduced in the mill while 35.5 parts by weight of the second are introduced at a uniform rate; The mixture as it issues from the mill should be passed through again, preferably twice at least, when the product will give a solution containing caustic soda of about 20% concentration.

9. Accelerators for the mdcam'zation of India rubber.In order to make a product consisting of china clay, zinc oxide or the like impregnated with an ingredient to form a'rubber accelerator, various processes are known in which liquid or gaseous ingredients combine to form a product for impregnating the china clay or zinc oxide. By introducing such ingredients into the mill together with the china clay pr zinc oxide reactions between them can be caused to take place simultaneously with the grinding up of the china clay or zifi c oxide into a finely divided form so that the finely divided product is uniformly impregnated with the in redients introduced by reaction. The following will serve as examples: 1.5 parts by weight of piperidene, 1.5 parts by weight ofcarbon bisulphide,.- and 31 parts by. weight of zinc oxide, are introduced into the mill either simultaneously, or in two lots consisting say of one-half of zinc oxide impregnated with piperidene and one-half impregnated with carbonbisulphide. The product is a useful rubber accelerator.

In another example, 6 parts by weight of china clay will replace the 31 parts by weight -of zinc oxide inthe first example.

zinc oxide impregnated with suiphur. it is Well known of course that, suiphur dioxide and hydrogen sulphide gases Wiii react to produce suipimin If chine ciey or the like is fed through the miii Whiic simultaneously screams of sulphur dioxide and hydrogen suiphide eie fed into the inlet of the miii through cipes, the gases Wiii iniimcieiymix in their passage through the iii to iocm suipimz' and this sciphcr is intimately mixed with the disintegrated chine clay or the iike so that e substeiniiciiy uniform product in a finely powdesed form issues from the mill.

In eii of cine examples above set forth it is the intense beating eciioc of the rotsiing stationary pins iii the miii combined with the forcing of ingredients iiir'oogh the miii in, c radici direction under the action of cootrifugai force, which insures the thorough disintegration endiniimcce intermixing' of the ingredien-is which renders their chemical reaction possible, It wiiibe fesiized, therefore, that the invention depends upon the use of a high speed centrifuge pinned disc miil in which the ingredients are introduced at the centre and are intimately mixed in their pessage radiaiiy through thc'miii between the pins,

Having chus descriified my invention what- ]i claim as new and desire to secure by Let;- tci's Pecos; is: i

in The recess of forming products by chemi'cai i'esciiocs which consists in mixing 'iifigilifi'ifliiilii reacting substances and subject chemical disintegration and "violent ceotrifu gel expcisive force chat they form a perms cent mixture and repidiy react direci-iy with one enothelx 2. The process of forming products icy ciiemicei ecc'cioos which consists mixing together the reacting substances, one at least of which is fluid end subjecting the mixici'e in such a high speed mechsnicei disinzegmfcion endviolene centrifugal .expuisivc force ems; the-solid substances remain permeneniiy in suspension in the fluid and react rapidly iiierewich.

3c The process of manufacturing soap which consists in adding cikeiiio a mixture of fatty acid and oil and subjecting the mixture to a, mechanical disintegration so such a iiigii speed and with such violent centrifugal expiiisive force that simultaneously tile alkali oeutcelizes the fatty acid seponifies the oil 2- process of manufacturing soap which consists in the mixing together oi oil and fatty acid in smelted condition, adding e soiution of alkali, subjecting said mixture to e iiigii speed mechanical disintegration and violent centrifugal expcisive force so that the oil becomes substsosiciiy seponified and the fatty acid neutralized while still in the ii uid condition and subset-in the mixcure to a second saege of such high SII'QGCi mechanical disintegration.

' JACQB WILLEAM SPENSLEY. 

